Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 131719752 | HCID 131719752 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131719751 | HCID 131719751 | 70% |
Reaction Steps
To a stirred solution of 4-(4'-methoxyphenyl)methylenehomophthalimide (279 mg, 1 mmol) in anhydrous dichloromethane (10 ml) is added at -78° C. under nitrogen, over a period of 10 min, a 1.0M solution of boron tribromide in dichloromethane (3 ml, 3 mmol). The resulting mixture is stirred for another 1 h at -78° C. and then allowed to warm to room temperature. After stirring for 1.5 h at 20°-25° C. the mixture is cooled to -10° C. and then quenched by dropwise addition of water (10 ml) over a 10-min period. After addition of ethyl acetate (10 ml) the organic layer is separated, washed with water, dried over Na2SO4 and evaporated under vacuum to dryness. The residue is crystallized from ethanol thus giving pure 4-(4'-hydroxyphenyl)methylenehomophthalimide (186 mg, yield 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05587385 |
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| Source dataset | uspto-grants-1996_12 |
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| ORD ID | ord-ccf90a10d12b429f8cbee9939770f81a |
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| Source note | uspto-grants-1996_12 |
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